CA2774231A1 - Composite material part having a ceramic matrix, and method for manufacturing same - Google Patents
Composite material part having a ceramic matrix, and method for manufacturing same Download PDFInfo
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- CA2774231A1 CA2774231A1 CA2774231A CA2774231A CA2774231A1 CA 2774231 A1 CA2774231 A1 CA 2774231A1 CA 2774231 A CA2774231 A CA 2774231A CA 2774231 A CA2774231 A CA 2774231A CA 2774231 A1 CA2774231 A1 CA 2774231A1
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- interphase
- phase
- ceramic matrix
- crack
- ceramic
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- 239000011159 matrix material Substances 0.000 title claims abstract description 115
- 239000000919 ceramic Substances 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 230000016507 interphase Effects 0.000 claims abstract description 137
- 239000000463 material Substances 0.000 claims abstract description 61
- 230000002787 reinforcement Effects 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims description 34
- 230000008021 deposition Effects 0.000 claims description 25
- 239000002243 precursor Substances 0.000 claims description 14
- 230000001737 promoting effect Effects 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- 229910010293 ceramic material Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 230000008030 elimination Effects 0.000 claims description 4
- 238000003379 elimination reaction Methods 0.000 claims description 4
- 239000002296 pyrolytic carbon Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 238000000280 densification Methods 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims description 2
- 239000012071 phase Substances 0.000 description 68
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 36
- 229910010271 silicon carbide Inorganic materials 0.000 description 36
- 239000011153 ceramic matrix composite Substances 0.000 description 17
- 239000000835 fiber Substances 0.000 description 14
- 239000007792 gaseous phase Substances 0.000 description 13
- 239000005055 methyl trichlorosilane Substances 0.000 description 11
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 11
- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 206010040844 Skin exfoliation Diseases 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007373 indentation Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000007596 consolidation process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000035876 healing Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 229910003465 moissanite Inorganic materials 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000001902 propagating effect Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 229920006184 cellulose methylcellulose Polymers 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 238000012710 chemistry, manufacturing and control Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/62873—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/6286—Carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
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- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/6286—Carbides
- C04B35/62863—Silicon carbide
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- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62884—Coating the powders or the macroscopic reinforcing agents by gas phase techniques
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62894—Coating the powders or the macroscopic reinforcing agents with more than one coating layer
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- C—CHEMISTRY; METALLURGY
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- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62897—Coatings characterised by their thickness
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- C—CHEMISTRY; METALLURGY
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
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- C—CHEMISTRY; METALLURGY
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- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
- C04B37/005—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts consisting of glass or ceramic material
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/614—Gas infiltration of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- C—CHEMISTRY; METALLURGY
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
- C04B2237/365—Silicon carbide
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/59—Aspects relating to the structure of the interlayer
- C04B2237/592—Aspects relating to the structure of the interlayer whereby the interlayer is not continuous, e.g. not the whole surface of the smallest substrate is covered by the interlayer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249924—Noninterengaged fiber-containing paper-free web or sheet which is not of specified porosity
- Y10T428/249928—Fiber embedded in a ceramic, glass, or carbon matrix
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Laminated Bodies (AREA)
- Ceramic Products (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
In a composite material part having a ceramic matrix and including a fibrous reinforcement which is densified by a matrix consisting of a plurality of ceramic layers having a crack-diverting matrix interphase positioned between two adjacent ceramic matrix layers, the interphase (10) includes: a first phase (12) made of a material conducive to the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase; and a second phase consisting of discrete contact pads (14) that are distributed within the interphase and conducive to the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
Description
Composite material part having a ceramic matrix, and method for manufacturing same Background of the invention The invention relates to composite material parts having a ceramic matrix, in particular, but not exclusively, parts for aeronautic engines or rocket engines.
Ceramic matrix composites (CMC) are made up of a fibrous reinforcement, in carbon or ceramic fibers, densified by a ceramic matrix. Their mechanical properties and temperature resistance make them suitable for use for structural parts exposed to high temperatures during use.
However, CMCs are subject to cracking under the effect of thermomechanical strains, often as of their production. In order to prevent the fibers of the fibrous reinforcement from breaking due to the cracks spreading through the matrix, and to prevent the rapid deterioration of the mechanical properties that would result therefrom, is well known to position an embrittlement relief interphase between the fibers and the matrix. Such an interphase is typically made from a material with a lamellar structure or texture which, when the crack reaches the interface, is capable of dissipating the cracking energy through a localized debonding so that the crack is diverted within the interphase. Component materials of an embrittlement relief interphase are in particular pyrolytic carbon PyC
and boron nitride BN, which have a lamellar structure.
Reference may be made to documents US 4 752 503 and US 5 026 604. Other materials can be used, for example such as boron-doped carbon BC and titanium silicocarbide Ti3SiC2.
Ceramic matrix composites (CMC) are made up of a fibrous reinforcement, in carbon or ceramic fibers, densified by a ceramic matrix. Their mechanical properties and temperature resistance make them suitable for use for structural parts exposed to high temperatures during use.
However, CMCs are subject to cracking under the effect of thermomechanical strains, often as of their production. In order to prevent the fibers of the fibrous reinforcement from breaking due to the cracks spreading through the matrix, and to prevent the rapid deterioration of the mechanical properties that would result therefrom, is well known to position an embrittlement relief interphase between the fibers and the matrix. Such an interphase is typically made from a material with a lamellar structure or texture which, when the crack reaches the interface, is capable of dissipating the cracking energy through a localized debonding so that the crack is diverted within the interphase. Component materials of an embrittlement relief interphase are in particular pyrolytic carbon PyC
and boron nitride BN, which have a lamellar structure.
Reference may be made to documents US 4 752 503 and US 5 026 604. Other materials can be used, for example such as boron-doped carbon BC and titanium silicocarbide Ti3SiC2.
2 In the case of use in a corrosive environment (oxidizing or humid medium), it is desirable to avoid easy access via cracking to the fibers of the reinforcement or to the fiber/matrix interphase when the fibers or interphase are made from a material, such as carbon, that is sensitive to such a corrosive environment.
To that end, it has been proposed to make the matrix at least partially through a self-healing ceramic phase made from a material capable, in the presence of oxygen, of forming a glass which, by passing into a fluid state at usage temperatures of the CMC material, can cause clogging or healing of cracks. A healing ceramic phase for example comprises the elements Si, B and C able to form a borosilicate glass. Reference may for example be made to document US 5 965 266.
It has also been proposed to dissipate the cracking energy within the matrix, before the cracks reach the fiber/matrix interphase, by forming the matrix from several ceramic layers while positioning a crack-diverting interphase between two adjacent matrix layers, the matrix phases also being able to be self-healing.
Reference may for example be made to documents US 5 074 039 and US 6 068 930.
However, the effectiveness of self-healing matrix phases is limited to a particular temperature range. The introduction of crack-deviating interfaces between matrix phases as proposed in the state of the art also has a limited effectiveness over time, the debondings created by the spread of the cracks in the interfaces being able to lead to peeling of the CMC material over time.
To that end, it has been proposed to make the matrix at least partially through a self-healing ceramic phase made from a material capable, in the presence of oxygen, of forming a glass which, by passing into a fluid state at usage temperatures of the CMC material, can cause clogging or healing of cracks. A healing ceramic phase for example comprises the elements Si, B and C able to form a borosilicate glass. Reference may for example be made to document US 5 965 266.
It has also been proposed to dissipate the cracking energy within the matrix, before the cracks reach the fiber/matrix interphase, by forming the matrix from several ceramic layers while positioning a crack-diverting interphase between two adjacent matrix layers, the matrix phases also being able to be self-healing.
Reference may for example be made to documents US 5 074 039 and US 6 068 930.
However, the effectiveness of self-healing matrix phases is limited to a particular temperature range. The introduction of crack-deviating interfaces between matrix phases as proposed in the state of the art also has a limited effectiveness over time, the debondings created by the spread of the cracks in the interfaces being able to lead to peeling of the CMC material over time.
3 Subject matter and brief description of the invention The invention therefore aims to provide a CMC part having a longer lifespan for use at a high temperature, up to at least 1000 C, and even up to at least 1200 C, in a corrosive environment.
This aim is achieved owing to a CMC part comprising a fibrous reinforcement which is densified by a matrix consisting of a plurality of ceramic layers having a crack-diverting matrix interphase positioned between two adjacent ceramic matrix layers, wherein the interphase includes:
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
In a CMC material comprising several matrix layers with an interphase positioned between two adjacent matrix layers, here we distinguish between a first crack propagation mode (or mode I) in the transverse direction in the matrix layers, and a second longitudinal propagation mode (mode II) along an interphase, within
This aim is achieved owing to a CMC part comprising a fibrous reinforcement which is densified by a matrix consisting of a plurality of ceramic layers having a crack-diverting matrix interphase positioned between two adjacent ceramic matrix layers, wherein the interphase includes:
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
In a CMC material comprising several matrix layers with an interphase positioned between two adjacent matrix layers, here we distinguish between a first crack propagation mode (or mode I) in the transverse direction in the matrix layers, and a second longitudinal propagation mode (mode II) along an interphase, within
4 the latter or at an interface between the interphase and an adjacent matrix layer.
The invention is remarkable for the capacity of the interphase to ensure deviate a crack reaching the interphase from an adjacent matrix phase by going from the first to the second propagation mode, followed by a redirection of the crack toward the other adjacent matrix phase by going from the second propagation mode back to the first propagation mode. In this way, the risk of peeling is reduced by limiting the extent of the debonding within the interphase layer and the resistance to the corrosive environment is extended by imposing a twisting journey on the cracks that extends the path through which the surrounding medium may potentially access the fibers of the fibrous reinforcement or a fiber/matrix interphase.
In one embodiment, the discrete contact pads making up the second phase perform localized bridging between the two ceramic matrix layers. The discrete contact pads then form a second binding phase by performing a mechanical connecting function between the matrix layers adjacent to the interphase. The discrete contact pads can be made from ceramic, for example silicon carbide SiC, another structural carbide, or a structural nitride, and can be formed integrally with one of the two adjacent ceramic matrix layers.
Preferably, the discrete contact pads occupy a surface fraction of the interphase of between 20% and 80%.
The material of the first phase of the interphase can be selected in the group made up of pyrolytic carbon PyC, boron nitride BN, boron-doped carbon BC, and a MAX
phase, in particular titanium silicocarbide Ti3SiC2.
^ CA 02774231 2012-03-14 Preferably, the interphase has a thickness of between 0.01 micron and 2 microns.
According to another aspect, the invention also aims to provide a method making it possible to produce a CMC
The invention is remarkable for the capacity of the interphase to ensure deviate a crack reaching the interphase from an adjacent matrix phase by going from the first to the second propagation mode, followed by a redirection of the crack toward the other adjacent matrix phase by going from the second propagation mode back to the first propagation mode. In this way, the risk of peeling is reduced by limiting the extent of the debonding within the interphase layer and the resistance to the corrosive environment is extended by imposing a twisting journey on the cracks that extends the path through which the surrounding medium may potentially access the fibers of the fibrous reinforcement or a fiber/matrix interphase.
In one embodiment, the discrete contact pads making up the second phase perform localized bridging between the two ceramic matrix layers. The discrete contact pads then form a second binding phase by performing a mechanical connecting function between the matrix layers adjacent to the interphase. The discrete contact pads can be made from ceramic, for example silicon carbide SiC, another structural carbide, or a structural nitride, and can be formed integrally with one of the two adjacent ceramic matrix layers.
Preferably, the discrete contact pads occupy a surface fraction of the interphase of between 20% and 80%.
The material of the first phase of the interphase can be selected in the group made up of pyrolytic carbon PyC, boron nitride BN, boron-doped carbon BC, and a MAX
phase, in particular titanium silicocarbide Ti3SiC2.
^ CA 02774231 2012-03-14 Preferably, the interphase has a thickness of between 0.01 micron and 2 microns.
According to another aspect, the invention also aims to provide a method making it possible to produce a CMC
5 part as defined above.
This aim is achieved owing to a method comprising the production of a fibrous preform and the densification of the fibrous preform by a matrix made up of several ceramic layers having a crack-deviating interphase placed between two adjacent ceramic matrix layers, in which the interphase is made with:
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
According to a first particular embodiment of the method, the interphase is made by co-deposition of the first phase and the second phase by chemical vapor infiltration.
According to a second particular embodiment of the method, the interphase is made by chemical vapor infiltration deposition on a ceramic matrix layer of a
This aim is achieved owing to a method comprising the production of a fibrous preform and the densification of the fibrous preform by a matrix made up of several ceramic layers having a crack-deviating interphase placed between two adjacent ceramic matrix layers, in which the interphase is made with:
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
According to a first particular embodiment of the method, the interphase is made by co-deposition of the first phase and the second phase by chemical vapor infiltration.
According to a second particular embodiment of the method, the interphase is made by chemical vapor infiltration deposition on a ceramic matrix layer of a
6 continuous layer of the material of the first phase, localized elimination of the material of the deposited layer to form a discontinuous layer, and filling in the spaces thus formed by depositing a material making up the second phase. The filling in of the spaces can be done by depositing a ceramic material during the formation of a subsequent ceramic matrix layer.
According to a third particular embodiment of the method, the interphase is made by discontinuous deposition on a ceramic matrix layer of a component material or precursor of the material of the first phase to form patches spaced apart from one another and filling in spaces between the patches by depositing a material making up the second phase. The filling in of the spaces can be done by ceramic material deposition during the formation of a subsequent ceramic matrix layer.
In this third embodiment of the method, it is possible to perform the discontinuous deposition by suspending, in a liquid carrier, particles of the component material or precursor of the material of the first phase; impregnating the ceramic matrix layer with the suspension; and eliminating the liquid binder to obtain particles dispersed on the surface of the ceramic matrix layer.
When the discontinuous deposition is formed by a precursor material of the material of the first phase, the transformation of the precursor material may occur by chemical reaction with a gas phase, during the formation of a subsequent ceramic matrix layer.
In a fourth embodiment of the method, the interphase is made through the formation, on a ceramic matrix layer, of nodules forming the discrete contact pads of the = CA 02774231 2012-03-14
According to a third particular embodiment of the method, the interphase is made by discontinuous deposition on a ceramic matrix layer of a component material or precursor of the material of the first phase to form patches spaced apart from one another and filling in spaces between the patches by depositing a material making up the second phase. The filling in of the spaces can be done by ceramic material deposition during the formation of a subsequent ceramic matrix layer.
In this third embodiment of the method, it is possible to perform the discontinuous deposition by suspending, in a liquid carrier, particles of the component material or precursor of the material of the first phase; impregnating the ceramic matrix layer with the suspension; and eliminating the liquid binder to obtain particles dispersed on the surface of the ceramic matrix layer.
When the discontinuous deposition is formed by a precursor material of the material of the first phase, the transformation of the precursor material may occur by chemical reaction with a gas phase, during the formation of a subsequent ceramic matrix layer.
In a fourth embodiment of the method, the interphase is made through the formation, on a ceramic matrix layer, of nodules forming the discrete contact pads of the = CA 02774231 2012-03-14
7 second phase, and the deposition of a layer of a material making up the first phase.
Brief description of the drawings The invention will be better understood upon reading the following description, provided for information but non-limitingly in reference to the appended drawings, in which:
- figure 1 very diagrammatically shows the propagation of a crack in the matrix of the CMC material having several ceramic matrix phases separated by embrittlement relief interphases according to the prior art;
- figure 2 very diagrammatically illustrates the propagation of a crack in the matrix of a CMC material according to the invention having several ceramic matrix phases separated by interphases;
- figure 3 very diagrammatically illustrates an example of an interphase according to the invention;
- figure 4A very diagrammatically illustrates another example of an interphase according to the invention, and figure 4B shows the propagation of a crack with redirection in such an interphase;
- figures 5A to 5C show the successive steps of a method for making an interphase like that of figure 4A;
- figures 6A and 6B shows successive steps of another method of making an interphase like that of figure 4A;
- figures 7A to 7C show the successive steps of still another method of making an interphase according to the invention;
- figure 8 is a scanning electron microscope view of a C+SiC co-deposit;
Brief description of the drawings The invention will be better understood upon reading the following description, provided for information but non-limitingly in reference to the appended drawings, in which:
- figure 1 very diagrammatically shows the propagation of a crack in the matrix of the CMC material having several ceramic matrix phases separated by embrittlement relief interphases according to the prior art;
- figure 2 very diagrammatically illustrates the propagation of a crack in the matrix of a CMC material according to the invention having several ceramic matrix phases separated by interphases;
- figure 3 very diagrammatically illustrates an example of an interphase according to the invention;
- figure 4A very diagrammatically illustrates another example of an interphase according to the invention, and figure 4B shows the propagation of a crack with redirection in such an interphase;
- figures 5A to 5C show the successive steps of a method for making an interphase like that of figure 4A;
- figures 6A and 6B shows successive steps of another method of making an interphase like that of figure 4A;
- figures 7A to 7C show the successive steps of still another method of making an interphase according to the invention;
- figure 8 is a scanning electron microscope view of a C+SiC co-deposit;
8 - figures 9 to 11 are scanning electron microscope views showing crack propagation modes;
- figure 12 is a scanning electron microscope view showing nodules formed on a surface of a ceramic phase;
and - figure 13 is a scanning electron microscope view showing an interphase according to the invention between two ceramic layers.
Detailed description of the invention Figure 1 very diagrammatically illustrates part of a known CMC material comprising several ceramic matrix layers or phases M1, M2r M3, M4 with an embrittlement relief interphase 112, 123, 134 positioned between two adjacent matrix layers. The interphases are made from a crack-deviating material, for example PyC, BN, BC or Ti3SiC2, so that a crack F reaching an interphase 112 by spreading transversely in an adjacent matrix layer M4 (crack propagation mode I) is deviated to continue its propagation along the interphase 134 through debonding within the latter or at an interface between the interphase 134 and an adjacent matrix layer M3 or M4 (crack propagation mode II).
In this way, the propagation of the crack through the entire matrix until it reaches the fibers of the CMC
material is avoided or delayed. However, the debonding corresponding to mode II propagation of course causes a risk of peeling of the CMC material.
Figure 2 very diagrammatically illustrates part of a CMC material according to the invention comprising several ceramic matrix layers or phases M1, M2, Mar M4 with a mixed interphase J12, J23, J34 positioned between
- figure 12 is a scanning electron microscope view showing nodules formed on a surface of a ceramic phase;
and - figure 13 is a scanning electron microscope view showing an interphase according to the invention between two ceramic layers.
Detailed description of the invention Figure 1 very diagrammatically illustrates part of a known CMC material comprising several ceramic matrix layers or phases M1, M2r M3, M4 with an embrittlement relief interphase 112, 123, 134 positioned between two adjacent matrix layers. The interphases are made from a crack-deviating material, for example PyC, BN, BC or Ti3SiC2, so that a crack F reaching an interphase 112 by spreading transversely in an adjacent matrix layer M4 (crack propagation mode I) is deviated to continue its propagation along the interphase 134 through debonding within the latter or at an interface between the interphase 134 and an adjacent matrix layer M3 or M4 (crack propagation mode II).
In this way, the propagation of the crack through the entire matrix until it reaches the fibers of the CMC
material is avoided or delayed. However, the debonding corresponding to mode II propagation of course causes a risk of peeling of the CMC material.
Figure 2 very diagrammatically illustrates part of a CMC material according to the invention comprising several ceramic matrix layers or phases M1, M2, Mar M4 with a mixed interphase J12, J23, J34 positioned between
9 two adjacent matrix layers. Each mixed interphase is formed by the juxtaposition of two phases:
- a first debonding phase made from a crack-deviating material capable of promoting the deviation of a crack reaching the interphase in mode I to mode II, and - a second phase made up of discrete contact pads (not shown in figure 2) capable of promoting the redirection of a crack propagating in mode II along the interphase into mode I.
In this way, a crack F reaching an interphase propagating in mode I through a ceramic matrix layer adjacent to the interphase is deviated to propagate in mode II along the interphase over a limited distance before being deviated again to continue its propagation in mode I through the other ceramic matrix layer adjacent to the interphase.
In this way, the risk of peeling is eliminated or at least greatly reduced. Furthermore, the winding path of the cracks makes it more difficult for corrosive species to reach the core of the material.
The mixed interphase can have a relatively small thickness, for example between 0.01 micron and 2 microns.
A mixed interphase offering a dual deviation capacity from mode I into mode II and redirection from mode II back to mode I can be made in different ways.
Producing a CMC material part with several matrix layers separated by interphases, in a known manner, comprises the following steps:
(a) making a fibrous preform having a shape corresponding to that of the part to be made, the preform being made from carbon or ceramic fibers, (b) forming a fiber/matrix embrittlement relief interphase layer on the fibers, said interphase layer possibly being able to be formed before producing the fibrous preform, (c) forming a ceramic matrix layer, (d) forming an interphase on the ceramic matrix 5 layer, (e) forming a ceramic matrix layer, and (f) possibly repeating steps (c) to (e) one or more times.
The fibrous preform can for example be obtained by
- a first debonding phase made from a crack-deviating material capable of promoting the deviation of a crack reaching the interphase in mode I to mode II, and - a second phase made up of discrete contact pads (not shown in figure 2) capable of promoting the redirection of a crack propagating in mode II along the interphase into mode I.
In this way, a crack F reaching an interphase propagating in mode I through a ceramic matrix layer adjacent to the interphase is deviated to propagate in mode II along the interphase over a limited distance before being deviated again to continue its propagation in mode I through the other ceramic matrix layer adjacent to the interphase.
In this way, the risk of peeling is eliminated or at least greatly reduced. Furthermore, the winding path of the cracks makes it more difficult for corrosive species to reach the core of the material.
The mixed interphase can have a relatively small thickness, for example between 0.01 micron and 2 microns.
A mixed interphase offering a dual deviation capacity from mode I into mode II and redirection from mode II back to mode I can be made in different ways.
Producing a CMC material part with several matrix layers separated by interphases, in a known manner, comprises the following steps:
(a) making a fibrous preform having a shape corresponding to that of the part to be made, the preform being made from carbon or ceramic fibers, (b) forming a fiber/matrix embrittlement relief interphase layer on the fibers, said interphase layer possibly being able to be formed before producing the fibrous preform, (c) forming a ceramic matrix layer, (d) forming an interphase on the ceramic matrix 5 layer, (e) forming a ceramic matrix layer, and (f) possibly repeating steps (c) to (e) one or more times.
The fibrous preform can for example be obtained by
10 shaping fibrous textures possibly in superimposed plies, such as sheets of threads, traditional two-dimensional (2D) fabrics or three-dimensional (3D) or multilayer fabrics.
In the case of a part to be made with a relatively complex shape, the fibrous preform may be consolidated to freeze it in the desired shape using a liquid method by impregnation using a consolidation composition containing a carbon or ceramic precursor resin, then curing and pyrolysis of the resin. A liquid consolidation process for preforms more particularly intended to produce CMC
parts is described in the French patent application filed under no. 0854937 by the applicant.
The fiber/matrix interphase layer, the interphases between ceramic matrix layers, as well as the ceramic matrix layers can be made by chemical vapor infiltration (CVI). To that end, the fibrous preform, possibly consolidated, is placed in an oven, and a reactive gaseous phase containing one or more precursors of the material to be deposited is introduced into the oven. The pressure and temperature conditions in particular are chosen to allow the gaseous phase to diffuse within the fibrous preform and form a desired deposit therein through decomposition of a component of the gaseous phase
In the case of a part to be made with a relatively complex shape, the fibrous preform may be consolidated to freeze it in the desired shape using a liquid method by impregnation using a consolidation composition containing a carbon or ceramic precursor resin, then curing and pyrolysis of the resin. A liquid consolidation process for preforms more particularly intended to produce CMC
parts is described in the French patent application filed under no. 0854937 by the applicant.
The fiber/matrix interphase layer, the interphases between ceramic matrix layers, as well as the ceramic matrix layers can be made by chemical vapor infiltration (CVI). To that end, the fibrous preform, possibly consolidated, is placed in an oven, and a reactive gaseous phase containing one or more precursors of the material to be deposited is introduced into the oven. The pressure and temperature conditions in particular are chosen to allow the gaseous phase to diffuse within the fibrous preform and form a desired deposit therein through decomposition of a component of the gaseous phase
11 or through reaction between several components. The composition of the reactive gaseous phase and, if applicable, the conditions for the CVI process (temperature, pressure, precursor level in the gaseous phase, residence time of the gaseous phase in the oven, etc.) are then modified during the transition of the deposition of a matrix layer in a given material to an interphase layer in another material (or vice versa).
Reference may be made to the documents cited at the beginning of the description regarding the production of embrittlement relief interphases or ceramic matrix layers by CVI.
As indicated below, the interphase may be at least partially made using a method other than a CVI process.
Figure 3 very diagrammatically illustrates a first embodiment of a mixed interphase 10 according to the invention between two ceramic matrix layers 20 and 30.
The interphase 10 comprises a first debonding phase
Reference may be made to the documents cited at the beginning of the description regarding the production of embrittlement relief interphases or ceramic matrix layers by CVI.
As indicated below, the interphase may be at least partially made using a method other than a CVI process.
Figure 3 very diagrammatically illustrates a first embodiment of a mixed interphase 10 according to the invention between two ceramic matrix layers 20 and 30.
The interphase 10 comprises a first debonding phase
12 in a material capable of promoting the diversion of a crack toward mode II by debonding, and a second phase 14 made up of grains or discrete contact pads capable. of promoting the redirection of the crack from mode II to mode I, the grains or contact pads of the phase 14 producing a bonding by localized bridging between the ceramic matrix layers 20 and 30.
The debonding phase 12 can for example be made from pyrolytic carbon PyC, boron nitride BN, boron-doped carbon BC (with between 5% at. and 20% at. B, the rest being C) or a MAX phase such as Ti3SiC2. The grains or contact pads forming the bonding phase 14 can be made from ceramic, for example silicon carbide SiC, another structural carbide or a structural nitride.
The interphase 10 can be obtained by co-deposition of phases 11 and 12 on the ceramic matrix layer 20. For example, a CVI co-deposition of a PyC phase 12 and a SiC
phase 14 can be done by using a reactive gaseous phase made up of methyltrichlorosilane (MTS) and hydrogen H2 with a very low ratio a between H2 rate and MTS rate, for example a < 1.
After formation of the interphase 10, the following ceramic layer 30 is formed. The matrix layers and the interphases are thus successively produced.
Figure 4 very diagrammatically illustrates another embodiment of a mixed interphase 110 according to the invention between two ceramic matrix layers 120 and 130.
The interphase comprises a first debonding phase 112 made from a material capable of diverting a crack toward mode II, and a second bonding phase 114 made up of discrete contact pads that produce a bonding by localized bridging between the layers of ceramic material while being formed with one of the matrix layers.
The first separating phase 112 can for example be made from PyC, BN, BC, or a MAX phase such as Ti3SiC2.
One method of forming the interphase 110 is shown by figures 5A to 5C.
After producing the matrix layer 120, a continuous layer 111 of debonding phase material is formed by CVI on the matrix layer 120 (figure 5A).
The layer 111 is locally eliminated to allow patches 112 separated from one another to remain (figure 5B). The local elimination of the layer 111 can be done by chemical or physical etching.
Then, the ceramic material of the layer 130 is deposited by CVI, in particular occupying the spaces between the patches 112 to form the contact pads 114.
The debonding phase 12 can for example be made from pyrolytic carbon PyC, boron nitride BN, boron-doped carbon BC (with between 5% at. and 20% at. B, the rest being C) or a MAX phase such as Ti3SiC2. The grains or contact pads forming the bonding phase 14 can be made from ceramic, for example silicon carbide SiC, another structural carbide or a structural nitride.
The interphase 10 can be obtained by co-deposition of phases 11 and 12 on the ceramic matrix layer 20. For example, a CVI co-deposition of a PyC phase 12 and a SiC
phase 14 can be done by using a reactive gaseous phase made up of methyltrichlorosilane (MTS) and hydrogen H2 with a very low ratio a between H2 rate and MTS rate, for example a < 1.
After formation of the interphase 10, the following ceramic layer 30 is formed. The matrix layers and the interphases are thus successively produced.
Figure 4 very diagrammatically illustrates another embodiment of a mixed interphase 110 according to the invention between two ceramic matrix layers 120 and 130.
The interphase comprises a first debonding phase 112 made from a material capable of diverting a crack toward mode II, and a second bonding phase 114 made up of discrete contact pads that produce a bonding by localized bridging between the layers of ceramic material while being formed with one of the matrix layers.
The first separating phase 112 can for example be made from PyC, BN, BC, or a MAX phase such as Ti3SiC2.
One method of forming the interphase 110 is shown by figures 5A to 5C.
After producing the matrix layer 120, a continuous layer 111 of debonding phase material is formed by CVI on the matrix layer 120 (figure 5A).
The layer 111 is locally eliminated to allow patches 112 separated from one another to remain (figure 5B). The local elimination of the layer 111 can be done by chemical or physical etching.
Then, the ceramic material of the layer 130 is deposited by CVI, in particular occupying the spaces between the patches 112 to form the contact pads 114.
13 Another method of forming the interphase 110 is shown by figures 6A and 6B.
After producing the ceramic matrix layer 120, patches 112a of a debonding phase material or a precursor material of the debonding phase material are formed on the layer 120 (figure 6A). The patches 112a are separated from one another.
To form the patches 112a, the following procedure may be used:
- preparation of a suspension in a liquid carrier of particles of the material of the debonding phase or of a precursor material of the material of the debonding phase, - impregnation of the matrix layer 120 by the suspension, and - elimination of the solid carrier to leave isolated particles dispersed on the surface of the matrix layer 120, while being anchored in the surface porosity of the layer 120, which always has a residual porosity, the particles having a size chosen not to exceed the thickness of the interphase to be produced.
The patches 112a can form the separating phase 112 either directly, or through chemical reaction with a gaseous phase brought in before the deposition of the following matrix layer 130 or by chemical reaction during the deposition of that matrix layer.
In this way, it is possible to form the patches 112a using titanium as the precursor that yields contact pads 112 made from Ti3SiC2 by reaction with an SiC gaseous precursor phase used to form the matrix layer 130.
The ceramic material of the matrix layer 130 is deposited by CVI, in particular occupying the spaces
After producing the ceramic matrix layer 120, patches 112a of a debonding phase material or a precursor material of the debonding phase material are formed on the layer 120 (figure 6A). The patches 112a are separated from one another.
To form the patches 112a, the following procedure may be used:
- preparation of a suspension in a liquid carrier of particles of the material of the debonding phase or of a precursor material of the material of the debonding phase, - impregnation of the matrix layer 120 by the suspension, and - elimination of the solid carrier to leave isolated particles dispersed on the surface of the matrix layer 120, while being anchored in the surface porosity of the layer 120, which always has a residual porosity, the particles having a size chosen not to exceed the thickness of the interphase to be produced.
The patches 112a can form the separating phase 112 either directly, or through chemical reaction with a gaseous phase brought in before the deposition of the following matrix layer 130 or by chemical reaction during the deposition of that matrix layer.
In this way, it is possible to form the patches 112a using titanium as the precursor that yields contact pads 112 made from Ti3SiC2 by reaction with an SiC gaseous precursor phase used to form the matrix layer 130.
The ceramic material of the matrix layer 130 is deposited by CVI, in particular occupying the spaces
14 between the patches 112a to form the contact pads 114 (figure 6B).
Figures 7A to 7C very diagrammatically illustrate still another method for producing a mixed interphase according to the invention.
Nodules 214 intended to form the discrete contact pads of the second phase of the interphase to be produced are deposited on a ceramic matrix layer 220 (figure 7A).
The nodules 214 can be obtained by chemical vapor deposition (CVD) by choosing deposition conditions yielding a discontinuous deposition formed by discrete nodules and not a continuous layer. In this way, for example, SiC or SiC+Si nodules can be obtained by using a gaseous phase comprising a mixture of MTS, H2, and hydrogen chloride HC1 with a ratio a between the H2 and MTS rates and a ratio 6 between the HC1 and MTS rates selected to that end, a preferably being comprised between 5 and 25, and 6 preferably being comprised between 0.05 and 2.
A continuous layer 211 of debonding phase is then formed by CVI on the matrix phase 220 and the nodules 214 (figure 7B) . The debonding phase can for example be made from PyC, BN, BC, or MAX phase such as Ti3SiC2. One thus obtains the matrix interphase 210 comprising the nodules 214 and the layer 211.
The following matrix layer 230 is then formed on the debonding phase 211.
The matrix phases 220 and 230 advantageously being formed by CVI, the production of the nodules 214 by CVD
makes it possible to link the steps for forming the matrix phases and the interphase in an oven by modifying the composition of the reactive gaseous phase.
The deposition on the matrix layer 220 of solid particles forming the second phase of the interphase could, however, be done by forming a suspension of small solid ceramic particles in a liquid carrier, for example 5 SiC, impregnating the matrix layer 220 with the suspension, and eliminating the liquid carrier to leave the ceramic particles dispersed on the surface of the matrix layer and anchored in the surface porosity.
Examples of the production of interphases will now 10 be described. In these examples, the interphases have been produced on monolithic substrates and not on composite substrates with fibrous reinforcements, the aim being to show the feasibility and the effects of the interphases.
Example 1 Produced on a silicon substrate was an assembly:
SiC/SiC+PyC interphase/SiC/SiC+PyC interphase/SiC, in which:
- the SiC layers are stoichiometric layers obtained by CVI in a well-known manner from a MTS+H2 gaseous phase at a temperature of approximately 1000 C and under a pressure of approximately 5 kPa, the ratio a between the H2 rate and the MTS rate being approximately 6, - the SiC+PyC interphases are obtained by CVI from a MTS+H2 gaseous phase yielding a first debonding phase PyC
with a lamellar structure and a second phase made up of PyC crystallites, the conditions being the same as those leading to the obtainment of stoichiometric SiC with the exception of the ratio a, which is chosen to be less than 1.
By choosing, for the formation of each interphase, a ratio a equal to approximately 0.1 (complete) and a duration of 1.5 min, an interphase was obtained with a thickness approximately equal to 30 nm containing 80% at.
of PyC, the rest being formed by SiC crystallites.
Figure 8 shows an obtained interphase, while figure 9 shows the path of a crack caused by indentation under a load. In figure 9, the circles indicate crack redirection zones (transitions from mode II to mode I).
Example 2 The same procedure was used as in example 1, but during the production of each interphase, with a ratio a approximately equal to 0.25 and a duration of 5 min., SiC+PyC interphases were obtained with a thickness approximately equal to 0.3 micron containing 70% at. of PyC, the rest being formed by SiC crystallites.
Figure 10 shows the path of a crack caused by indentation under a load. One can see an absence of transition from mode I to mode II in the second interphase, such a transition with redirection into mode I occurring in the first interphase.
Example 3 The same procedure was used as in example 1, but during the production of each interphase, with a ratio a approximately equal to 0.5 and a duration of 5 min., SiC+PyC interphases were obtained with a thickness approximately equal to 0.2 micron containing 60% at. of PyC, the rest being formed by SiC crystallites.
Figure 11 shows the path of a crack caused by indentation under a load. One can see an absence of transition from mode I to mode II in both interphases, reflecting the insufficient presence of a debonding phase.
Example 4 SiC+Si (non-stoichiometric SiC highly enriched with Si) nodules were formed by CVD on a SiC substrate using a gaseous MTS+H2+HC1 phase, at a temperature of approximately 1000 C, under a pressure of approximately 5 kPa and with a and 6 rate ratios equal to approximately 8 and approximately 0.5, respectively, the deposition time being approximately 30 min.
Figure 12 shows the obtained SiC+Si nodules. They have an average diameter of approximately 300 nm and an average height of approximately 100 nm and the mean distance between nodules is approximately 5 microns.
Example 5 Produced on a silicon substrate was an assembly:
SiC/(SiC+Si)+PyC interphase/SiC, in which:
- the SiC layers are stoichiometric SiC layers obtained by CVI as in example 1, - the (SiC+Si)+PyC interphase is obtained by CVD
deposition of discrete SiC+Si nodules, then CVI
deposition of a continuous PyC layer.
The CVD deposition of the SiC+Si nodules (non-stoichiometric SiC highly enriched with Si) was obtained by using a gaseous MTS+H2+HC1 phase, at a temperature of approximately 1000 C, under a pressure of approximately 5 kPa and with a and 6 rate ratios equal to approximately 20 and approximately 0.5, respectively, the deposition time being approximately 30 min.
The deposition of the continuous PyC layer was obtained by using a gaseous phase containing propane, at a temperature of about 1000 C, under a pressure of about 5 kPa, the deposition time being about 2.5 min.
Figure 13 shows the obtained interphase with a mean thickness approximately equal to 50 nm.
Figures 7A to 7C very diagrammatically illustrate still another method for producing a mixed interphase according to the invention.
Nodules 214 intended to form the discrete contact pads of the second phase of the interphase to be produced are deposited on a ceramic matrix layer 220 (figure 7A).
The nodules 214 can be obtained by chemical vapor deposition (CVD) by choosing deposition conditions yielding a discontinuous deposition formed by discrete nodules and not a continuous layer. In this way, for example, SiC or SiC+Si nodules can be obtained by using a gaseous phase comprising a mixture of MTS, H2, and hydrogen chloride HC1 with a ratio a between the H2 and MTS rates and a ratio 6 between the HC1 and MTS rates selected to that end, a preferably being comprised between 5 and 25, and 6 preferably being comprised between 0.05 and 2.
A continuous layer 211 of debonding phase is then formed by CVI on the matrix phase 220 and the nodules 214 (figure 7B) . The debonding phase can for example be made from PyC, BN, BC, or MAX phase such as Ti3SiC2. One thus obtains the matrix interphase 210 comprising the nodules 214 and the layer 211.
The following matrix layer 230 is then formed on the debonding phase 211.
The matrix phases 220 and 230 advantageously being formed by CVI, the production of the nodules 214 by CVD
makes it possible to link the steps for forming the matrix phases and the interphase in an oven by modifying the composition of the reactive gaseous phase.
The deposition on the matrix layer 220 of solid particles forming the second phase of the interphase could, however, be done by forming a suspension of small solid ceramic particles in a liquid carrier, for example 5 SiC, impregnating the matrix layer 220 with the suspension, and eliminating the liquid carrier to leave the ceramic particles dispersed on the surface of the matrix layer and anchored in the surface porosity.
Examples of the production of interphases will now 10 be described. In these examples, the interphases have been produced on monolithic substrates and not on composite substrates with fibrous reinforcements, the aim being to show the feasibility and the effects of the interphases.
Example 1 Produced on a silicon substrate was an assembly:
SiC/SiC+PyC interphase/SiC/SiC+PyC interphase/SiC, in which:
- the SiC layers are stoichiometric layers obtained by CVI in a well-known manner from a MTS+H2 gaseous phase at a temperature of approximately 1000 C and under a pressure of approximately 5 kPa, the ratio a between the H2 rate and the MTS rate being approximately 6, - the SiC+PyC interphases are obtained by CVI from a MTS+H2 gaseous phase yielding a first debonding phase PyC
with a lamellar structure and a second phase made up of PyC crystallites, the conditions being the same as those leading to the obtainment of stoichiometric SiC with the exception of the ratio a, which is chosen to be less than 1.
By choosing, for the formation of each interphase, a ratio a equal to approximately 0.1 (complete) and a duration of 1.5 min, an interphase was obtained with a thickness approximately equal to 30 nm containing 80% at.
of PyC, the rest being formed by SiC crystallites.
Figure 8 shows an obtained interphase, while figure 9 shows the path of a crack caused by indentation under a load. In figure 9, the circles indicate crack redirection zones (transitions from mode II to mode I).
Example 2 The same procedure was used as in example 1, but during the production of each interphase, with a ratio a approximately equal to 0.25 and a duration of 5 min., SiC+PyC interphases were obtained with a thickness approximately equal to 0.3 micron containing 70% at. of PyC, the rest being formed by SiC crystallites.
Figure 10 shows the path of a crack caused by indentation under a load. One can see an absence of transition from mode I to mode II in the second interphase, such a transition with redirection into mode I occurring in the first interphase.
Example 3 The same procedure was used as in example 1, but during the production of each interphase, with a ratio a approximately equal to 0.5 and a duration of 5 min., SiC+PyC interphases were obtained with a thickness approximately equal to 0.2 micron containing 60% at. of PyC, the rest being formed by SiC crystallites.
Figure 11 shows the path of a crack caused by indentation under a load. One can see an absence of transition from mode I to mode II in both interphases, reflecting the insufficient presence of a debonding phase.
Example 4 SiC+Si (non-stoichiometric SiC highly enriched with Si) nodules were formed by CVD on a SiC substrate using a gaseous MTS+H2+HC1 phase, at a temperature of approximately 1000 C, under a pressure of approximately 5 kPa and with a and 6 rate ratios equal to approximately 8 and approximately 0.5, respectively, the deposition time being approximately 30 min.
Figure 12 shows the obtained SiC+Si nodules. They have an average diameter of approximately 300 nm and an average height of approximately 100 nm and the mean distance between nodules is approximately 5 microns.
Example 5 Produced on a silicon substrate was an assembly:
SiC/(SiC+Si)+PyC interphase/SiC, in which:
- the SiC layers are stoichiometric SiC layers obtained by CVI as in example 1, - the (SiC+Si)+PyC interphase is obtained by CVD
deposition of discrete SiC+Si nodules, then CVI
deposition of a continuous PyC layer.
The CVD deposition of the SiC+Si nodules (non-stoichiometric SiC highly enriched with Si) was obtained by using a gaseous MTS+H2+HC1 phase, at a temperature of approximately 1000 C, under a pressure of approximately 5 kPa and with a and 6 rate ratios equal to approximately 20 and approximately 0.5, respectively, the deposition time being approximately 30 min.
The deposition of the continuous PyC layer was obtained by using a gaseous phase containing propane, at a temperature of about 1000 C, under a pressure of about 5 kPa, the deposition time being about 2.5 min.
Figure 13 shows the obtained interphase with a mean thickness approximately equal to 50 nm.
Claims (15)
1. A composite material part having a ceramic matrix and comprising a fibrous reinforcement which is densified by a matrix consisting of a plurality of ceramic layers having a crack-diverting matrix interphase positioned between two adjacent ceramic matrix layers, characterized in that the interphase (10; 110; 210) includes:
a first phase (12; 112; 211) made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads (14; 114; 214) that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
a first phase (12; 112; 211) made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads (14; 114; 214) that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
2. A part according to claim 1, characterized in that the discrete contact pads making up the second phase perform localized bridging between the two ceramic matrix layers.
3. A part according to claim 2, characterized in that the discrete contact pads are made from ceramic.
4. A part according to claim 3, characterized in that the discrete contact pads are formed integrally with one of the two adjacent ceramic matrix layers.
5. A part according to any one of claims 1 to 4, characterized in that the discrete contact pads occupy a surface fraction of the interphase of between 20% and 80%.
6. A part according to any one of claims 1 to 5, characterized in that the material of the first phase of the interphase is selected in the group made up of pyrolytic carbon PyC, boron nitride BN, boron-doped carbon BC, and a MAX phase, in particular titanium silicocarbide Ti3SiC2.
7. A part according to any one of claims 1 to 6, characterized in that the interphase has a thickness of between 0.01 micron and 2 microns.
8. A method for producing a composite material part having a ceramic matrix, comprising the production of a fibrous preform and the densification of the fibrous preform by a matrix made up of several ceramic layers having a crack-deviating interphase placed between two adjacent ceramic matrix layers, in which the interphase is made with:
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
a first phase made of a material capable of promoting the diversion of a crack reaching the interphase according to a first propagation mode in the transverse direction through one of the two ceramic matrix layers adjacent to the interphase, such that the propagation of the crack continues according to a second propagation mode along the interphase, and a second phase consisting of discrete contact pads that are distributed within the interphase and capable of promoting the diversion of the crack that propagates along the interphase according to the second propagation mode, such that the propagation of the crack is diverted and continues according to the first propagation mode through the other ceramic matrix layer that is adjacent to the interphase.
9. A method according to claim 8, characterized in that the interphase is made by co-deposition of the first phase and the second phase by chemical vapor infiltration.
10. A method according to claim 8, characterized in that the interphase is made by chemical vapor infiltration deposition on a ceramic matrix layer of a continuous layer of the material of the first phase, localized elimination of the material of the deposited layer to form a discontinuous layer, and filling in the spaces thus formed by depositing a material making up the second phase.
11. A method according to claim 8, characterized in that the interphase is made by discontinuous deposition on a ceramic matrix layer of a component material or precursor of the material of the first phase to form patches spaced apart from one another and filling in spaces between the patches by depositing a material making up the second phase.
12. A method according to claim 11, characterized in that the discontinuous deposition is carried out by suspending, in a liquid carrier, particles of the component material or precursor of the material of the first phase; impregnating the ceramic matrix layer with the suspension; and eliminating the liquid carrier to obtain particles dispersed on the surface of the ceramic matrix layer.
13. A method according to any one of claims 10 and 11, characterized in that the discontinuous deposition is formed by a precursor material of the material of the first phase, and the transformation of the precursor material is done by chemical reaction with a gas phase, during the formation of a subsequent ceramic matrix layer.
14. A method according to any one of claims 10 to 13, characterized in that the filling in of the spaces is done by ceramic material deposition during the formation of a subsequent ceramic matrix layer.
15. A method according to claim 8, characterized in that the interphase is made through the formation, on a ceramic matrix layer, of nodules forming the discrete contact pads of the second phase, and the deposition of a layer of a material making up the first phase.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR0956694 | 2009-09-28 | ||
| FR0956694A FR2950622B1 (en) | 2009-09-28 | 2009-09-28 | PIECE OF COMPOSITE MATERIAL WITH CERAMIC MATRIX AND METHOD FOR MANUFACTURING THE SAME |
| PCT/FR2010/051545 WO2011036358A1 (en) | 2009-09-28 | 2010-07-21 | Composite material part having a ceramic matrix, and method for manufacturing same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2774231A1 true CA2774231A1 (en) | 2011-03-31 |
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ID=42084609
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2774231A Abandoned CA2774231A1 (en) | 2009-09-28 | 2010-07-21 | Composite material part having a ceramic matrix, and method for manufacturing same |
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| Country | Link |
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| US (1) | US20120164430A1 (en) |
| EP (1) | EP2483073B1 (en) |
| JP (1) | JP5722330B2 (en) |
| KR (1) | KR101701545B1 (en) |
| CN (1) | CN102470630B (en) |
| BR (1) | BR112012000853A2 (en) |
| CA (1) | CA2774231A1 (en) |
| FR (1) | FR2950622B1 (en) |
| RU (1) | RU2531394C2 (en) |
| WO (1) | WO2011036358A1 (en) |
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| WO2014159557A1 (en) * | 2013-03-14 | 2014-10-02 | Rolls-Royce Corporation | Multi-layer fiber coating containing a sic and bn coating layer |
| EP4353701A3 (en) | 2013-11-26 | 2024-07-24 | RTX Corporation | Gas turbine engine component coating with self-healing barrier layer |
| US9470603B2 (en) * | 2014-04-25 | 2016-10-18 | Teledyne Scientific & Imaging, Llc | Morphing ceramic composite components for hypersonic wind tunnel |
| US10501378B2 (en) * | 2015-02-24 | 2019-12-10 | United Technologies Corporation | Conformal composite coatings and methods |
| CA2939288A1 (en) * | 2015-08-28 | 2017-02-28 | Rolls-Royce High Temperature Composites, Inc. | Ceramic matrix composite including silicon carbide fibers in a ceramic matrix comprising a max phase compound |
| US10801108B2 (en) * | 2017-08-28 | 2020-10-13 | Raytheon Technologies Corporation | Method for fabricating ceramic matrix composite components |
| CN108585907B (en) * | 2018-05-03 | 2021-09-14 | 中国航发北京航空材料研究院 | Cr (chromium)2Preparation method of AlC modified self-healing silicon carbide ceramic matrix composite |
| CN109608217B (en) * | 2018-12-13 | 2021-09-03 | 湖南泽睿新材料有限公司 | SiC containing MAX phase interface layerfPreparation method of/SiC composite material |
| US11506383B2 (en) * | 2020-10-09 | 2022-11-22 | Pratt & Whitney Canada Corp | Combustor liner and method of operating same |
| DE102022202475A1 (en) | 2022-03-11 | 2023-09-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein | Multi-layer material composite, component comprising the multi-layer material composite, method for their production and their use |
| FR3141167A1 (en) * | 2022-10-21 | 2024-04-26 | Safran Ceramics | Process for manufacturing a part made of ceramic matrix composite material |
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| FR2567874B1 (en) | 1984-07-20 | 1987-01-02 | Europ Propulsion | PROCESS FOR MANUFACTURING A COMPOSITE MATERIAL WITH REFRACTORY FIBROUS REINFORCEMENT AND CERAMIC MATRIX, AND STRUCTURE AS OBTAINED BY THIS PROCESS |
| US4956137A (en) * | 1986-09-16 | 1990-09-11 | Lanxide Technology Company, Lp | Porous ceramic composite with dense surface |
| US5290491A (en) * | 1990-04-02 | 1994-03-01 | Societe Europeenne De Propulsion | Process for the manufacture of a thermostructural composite material having a carbon interphase between its reinforcement fibers and its matrix |
| US5074039A (en) | 1990-10-26 | 1991-12-24 | Amp Incorporated | Method of manufacturing electrical connectors |
| FR2668477B1 (en) * | 1990-10-26 | 1993-10-22 | Propulsion Ste Europeenne | REFRACTORY COMPOSITE MATERIAL PROTECTED AGAINST CORROSION, AND METHOD FOR THE PRODUCTION THEREOF. |
| RU2045500C1 (en) * | 1992-11-19 | 1995-10-10 | Московский авиационный технологический институт им.К.Э.Циолковского | Method for production of ceramic composite |
| FR2732338B1 (en) * | 1995-03-28 | 1997-06-13 | Europ Propulsion | COMPOSITE MATERIAL PROTECTED AGAINST OXIDATION BY SELF-HEALING MATRIX AND MANUFACTURING METHOD THEREOF |
| FR2732962B1 (en) * | 1995-04-12 | 1997-07-04 | Europ Propulsion | PROCESS FOR CHEMICAL VAPOR INFILTRATION OF A MATERIAL COMPOSED OF CARBON AND SILICON AND / OR BORON |
| FR2742433B1 (en) | 1995-12-14 | 1998-03-13 | Europ Propulsion | THERMOSTRUCTURAL COMPOSITE MATERIALS WITH CARBON FIBER REINFORCEMENTS OR CARBON COATED, HAVING INCREASED OXIDATION RESISTANCE |
| US6979490B2 (en) | 2001-01-16 | 2005-12-27 | Steffier Wayne S | Fiber-reinforced ceramic composite material comprising a matrix with a nanolayered microstructure |
| FR2882356B1 (en) * | 2005-02-23 | 2008-08-15 | Snecma Propulsion Solide Sa | METHOD FOR MANUFACTURING PIECE OF COMPOSITE MATERIAL WITH CERAMIC MATRIX AND PART THUS OBTAINED |
| FR2907117B1 (en) | 2006-10-17 | 2010-09-24 | Snecma Propulsion Solide | PROCESS FOR MANUFACTURING A COMPOSITE MATERIAL PART WITH A CERAMIC MATRIX CONTAINING CRACKING MATRIX PHASES AND A CRACKING DEVIATOR |
| CN101033137A (en) * | 2007-02-06 | 2007-09-12 | 西北工业大学 | Method of preparing carbon/carbon-silicon carbide ceramics base composite material |
| FR2933970B1 (en) * | 2008-07-21 | 2012-05-11 | Snecma Propulsion Solide | METHOD FOR MANUFACTURING A PIECE OF THERMOSTRUCTURAL COMPOSITE MATERIAL AND PIECE THUS OBTAINED |
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- 2009-09-28 FR FR0956694A patent/FR2950622B1/en not_active Expired - Fee Related
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- 2010-07-21 WO PCT/FR2010/051545 patent/WO2011036358A1/en active Application Filing
- 2010-07-21 BR BR112012000853A patent/BR112012000853A2/en not_active IP Right Cessation
- 2010-07-21 CN CN201080031305.9A patent/CN102470630B/en not_active Expired - Fee Related
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| JP5722330B2 (en) | 2015-05-20 |
| KR20120079834A (en) | 2012-07-13 |
| EP2483073A1 (en) | 2012-08-08 |
| EP2483073B1 (en) | 2015-04-08 |
| US20120164430A1 (en) | 2012-06-28 |
| CN102470630B (en) | 2014-09-10 |
| FR2950622A1 (en) | 2011-04-01 |
| WO2011036358A1 (en) | 2011-03-31 |
| CN102470630A (en) | 2012-05-23 |
| JP2013505857A (en) | 2013-02-21 |
| RU2531394C2 (en) | 2014-10-20 |
| RU2012114237A (en) | 2013-11-10 |
| FR2950622B1 (en) | 2011-10-21 |
| KR101701545B1 (en) | 2017-02-01 |
| BR112012000853A2 (en) | 2016-03-01 |
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